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Preparation method of bimetallic catalyst and application of bimetallic catalyst in in allyl ether synthesis

A bimetallic catalyst and allyl ether technology, applied in the field of catalyst synthesis, can solve the problems that the catalyst cannot be reused, the low yield is not suitable for industrial production, and is toxic, so as to meet the needs of large-scale industrial production and long-term production , The effect of simple process route

Active Publication Date: 2021-01-12
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the above methods have their own disadvantages, for example: the first production method will produce a large amount of hydrogen chloride to corrode the equipment, which greatly increases the cost; the catalyst in the second production method cannot be reused; the third production method is only suitable for aromatic alcohols
[0004] In addition, Japanese patent JP60252400 has introduced a kind of preparation method of trimethylolpropane diallyl ether with trimethylolpropane and allyl chloride, but its yield is low and is not suitable for industrialized production; U.S. Patent US3355502 introduces A method for the preparation of allyl ethers from hydroxyalkanes and allyl alcohols using Hg + And BF as catalyst, use benzene as reaction medium, but this reaction catalyst and reaction medium are poisonous, subsequent separation will increase production cost
[0005] At present, there is no solution to the above problems in the prior art, and the production cost of allyl ether is relatively high, so a new process is urgently needed to solve the above problems

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Catalyst preparation

[0036] 80.0g (1.0mol) of TiO 2 Add to containing (NH 4 ) 6 (Mo 7 )O 24 (H 2 O) 4 (49.0g, 0.04mol) in a 10% dilute aqueous solution, impregnated for 30 minutes, dried the impregnated mixture at 110°C for 3 hours, and then dried at 5°C in air -1 The heating rate was increased from 110°C to 500°C for calcination, and after the temperature was raised to 500°C, the calcination was continued at this temperature for 3 hours, and finally 87.32g of bimetallic catalyst was obtained. According to the elemental analysis, the chemical formula was TiMoO 4 .

[0037] Elemental analysis: Ti: 23.0%, O: 30.8%, Mo: 46.2%;

[0038] Synthesis of 1,3-Propanediol Diallyl Ether (Wilson Synthesis)

[0039] Add 760.0g (10mol) of 1,3-propanediol and 1740.0g (30mol) allyl alcohol into a 5L reactor, then add 76.0g of the above-mentioned bimetallic catalyst, replace the reactor with nitrogen for 3 times, and seal the reactor. Heated to 145°C, reacted for 3 hours, coole...

Embodiment 2

[0042] Catalyst preparation

[0043] 80.0g (1.0mol) of TiO 2 Added to MgMoO 4 (18.4g, 0.1mol) in a 15% dilute aqueous solution, after impregnating for 5h, the impregnated mixture was dried at 50°C for 5 hours, and then dried in air at 10°C min -1 The heating rate was increased from 50°C to 600°C for calcination, and after the temperature was raised to 600°C, the calcination was continued at this temperature for 3 hours, and finally 91.4g of bimetallic catalyst was obtained. According to the elemental analysis, the chemical formula was TiMo 0.5 o 2 .

[0044] Elemental analysis: Ti: 37.6%, O: 25.0%, Mo: 37.4%

[0045] Synthesis of Diallyl Ether of Bisphenol A

[0046] The bisphenol A of 2282.9g (10mol) and 2320.0g (40mol) allyl alcohol are joined in the 10L reactor, then add 228.3.0g bimetallic catalyst, after nitrogen replacement 3 times, reactor is sealed, and reactor is heated to Reacted at 150°C for 3 hours, cooled to room temperature, poured out the reactant, filtere...

Embodiment 3

[0049] Catalyst preparation

[0050] 80.0g (1.0mol) of TiO 2 added to Na 2 MoO 4 (10.3g, 0.05mol) in a 20% dilute aqueous solution, after immersion for 10h, the impregnated mixture was dried at 150°C for 2 hours, and then dried at 10°C in air -1 The heating rate was increased from 150°C to 450°C for calcination, and after the temperature was raised to 450°C, the calcination was continued at this temperature for 3 hours, and finally 84.8g of bimetallic catalyst was obtained. According to the elemental analysis, the chemical formula was TiMo 0.2 o 2 .

[0051] Elemental analysis: Ti: 48.4%, O: 32.3%, Mo: 19.3%

[0052] Synthesis of Allyl Butyl Ether

[0053] Add 741.2g (10mol) of butanol and 871.2g (15mol) of allyl alcohol into a 3L reactor, then add 80.65g of a bimetallic catalyst, replace the reactor with nitrogen for 3 times, and heat the reactor to 150°C , reacted for 3 hours, cooled to room temperature, poured out the reactant, filtered out the catalyst, washed with ...

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PUM

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Abstract

The invention discloses a preparation method of a bimetallic catalyst and application of the bimetallic catalyst in allyl ether synthesis, the molecular formula of the bimetallic catalyst is TiMoxOy,allyl alcohol and one or more selected from monohydric alcohol, polyhydric alcohol and monohydric phenol are used as raw materials, and an allyl ether compound can be prepared through adoption of a Wilson synthesis method in the presence of the bimetallic catalyst. By using the bimetallic catalyst, the defects that the catalyst is difficult to recover and the byproduct haloid acid corrodes equipment are overcome, a solvent is not required to be added in the synthesis process, and the product yield is greater than 96%, so that the production cost is greatly reduced.

Description

technical field [0001] The invention belongs to the technical field of catalyst synthesis, and in particular relates to a preparation method of a bimetallic catalyst and its application in synthesizing allyl ether. Background technique [0002] As we all know, allyl ether is a useful part of industrial production and laboratory synthesis. The structure of allyl ether has the properties of isomerization, oxygen binding and polymerization, and is often used in protecting groups, polymer monomers or crosslinking agents, and photocatalysts. Curing, thermal curing, free radical curing coatings and air-drying unsaturated polyester coatings, flame retardant resins and other fields. [0003] There are roughly three methods for producing allyl ethers: (1) Allyl halides react with corresponding alcohols to generate allyl ethers under the catalysis of a base; Propanol reacts directly with alcohol to generate allyl ether; (3) in CSmHnPW 12 o 40 / ZrO 2 Under the condition of catalyst...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/28B01J37/02B01J37/08C07C41/09C07C43/15C07C43/205
CPCB01J23/28B01J23/002B01J37/0201B01J37/088C07C41/09C07C43/15C07C43/2055
Inventor 刘喆刘超许振成董龙跃赵聪牟通
Owner WANHUA CHEM GRP CO LTD